U.S. patent number 5,368,847 [Application Number 07/809,761] was granted by the patent office on 1994-11-29 for stable emulsions of perfluoropolyethers and fat substances and process for preparing them.
This patent grant is currently assigned to Ausimont S.p.A.. Invention is credited to Fabio Brunetta, Giovanni Pantini.
United States Patent |
5,368,847 |
Brunetta , et al. |
November 29, 1994 |
Stable emulsions of perfluoropolyethers and fat substances and
process for preparing them
Abstract
The invention relates to stable emulsions of perfluoropolyethers
having perfluoroalkyl end groups and of fat substances, consisting
of: one or more perfluoropolyethers having perfluoroalkyl end
groups: 1-50% by weight, one or more polyhydroxylated compounds
selected from glycerol and polyalcohols other than glycerol and
saccharides, containing at least three hydroxylic groups, said
compounds being dissolved in water or in a hydrophilic solvent when
they are solid: 10-95% by weight, including water and the
hydrophilic solvent, if any, one or more fat substances having a
melting temperature not higher than 100.degree. C.: 10-80% by
weight, one or more emulsifiers: 0.1-10% by weight. These emulsions
are utilized, in particular, in cosmetology and dermatology.
Inventors: |
Brunetta; Fabio (Cornuda,
IT), Pantini; Giovanni (Milan, IT) |
Assignee: |
Ausimont S.p.A. (Milan,
IT)
|
Family
ID: |
25675019 |
Appl.
No.: |
07/809,761 |
Filed: |
December 18, 1991 |
Foreign Application Priority Data
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Dec 18, 1990 [IT] |
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22415 A/90 |
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Current U.S.
Class: |
424/61; 424/401;
424/59; 424/63; 424/64; 514/844; 514/937; 516/20 |
Current CPC
Class: |
A61K
8/06 (20130101); A61K 8/70 (20130101); A61Q
19/00 (20130101); C08J 3/03 (20130101); C08J
3/09 (20130101); A61Q 17/00 (20130101); A61Q
17/04 (20130101); C08J 2371/00 (20130101); Y10S
514/844 (20130101); Y10S 514/937 (20130101) |
Current International
Class: |
A61K
8/70 (20060101); A61K 8/30 (20060101); C08J
3/03 (20060101); C08J 3/02 (20060101); C08J
3/09 (20060101); A61K 007/02 (); A61K
007/027 () |
Field of
Search: |
;424/401,63,59,64,78.03
;514/844,937 ;252/DIG.5 |
References Cited
[Referenced By]
U.S. Patent Documents
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4803067 |
February 1989 |
Brunetta et al. |
5093023 |
March 1992 |
Pantini et al. |
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Foreign Patent Documents
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0196904 |
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Mar 1986 |
|
EP |
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0390206 |
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Mar 1990 |
|
EP |
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Primary Examiner: Page; Thurman K.
Assistant Examiner: Hulina; Amy
Attorney, Agent or Firm: Cave; Bryan
Claims
What we claim is:
1. Stable emulsions of a first dispersed phase consisting of a
perfluoropolyether or perfluoropolyethers having perfluoroalkyl end
groups and of a second dispersed phase consisting of one or more
fat substances having a melting temperature not higher than
100.degree. C., said two phases being dispersed in a continuous
phase consisting of one or more polyhydroxylated compounds selected
from glycerol and polyalcohols other than glycerol and saccharides,
containing at least three hydroxyl groups, said emulsions having
the following weight composition:
(a) perfluoropolyether or perfluoropolyethers: 1-50% by weight of
the emulsion,
(b) polyhydroxylated compound or compounds: 10-95% by weight of the
emulsion,
(c) fat substance or substances: 10-80% by weight of the emulsion,
and
(d) one or more emulsifiers which are soluble in the
polyhydroxylated compound or compounds: 0.1-10% by weight of the
emulsion.
2. The stable emulsions according to claim 1, wherein the
perfluoropolyether or perfluoropolyethers have a number average
molecular weight ranging from 500 to 20,000.
3. The stable emulsions according to claim 1, wherein the
polyhydroxylated compounds are selected from diglycerol,
triglycerine and tetraglycerine.
4. The stable emulsions according to claim 1, wherein the fat
substances are selected from the group consisting of fat alcohols,
acids, esters and amides, silicone oils, hydrocarbon oils and
fats.
5. The stable emulsions according to claim 1 wherein the
emulsifiers are ionic.
6. The stable emulsions according to claim 12, consisting of:
(a) 5-25% by weight of the emulsion of one or more
perfluoropolyethers having perfluoroalkyl end groups, and
(b) 10-59% by weight of the emulsion of one or more
polyhydroxylated compounds, and
(c) 35-80% by weight of the emulsion of one or more fat substances,
and
(d) 0.3-3% by weight of the emulsion of one or more
emulsifiers.
7. The stable emulsions according to claim 6, containing from 10 to
40% by weight of one or more polyhydroxylated compounds.
8. A process for preparing the stable emulsions of claim 1,
comprising adding one or more fat substances in the liquid state
under stirring to a pre-emulsion of one or more perfluoropolyethers
in one or more polyhydroxylated compounds, containing one or more
emulsifiers which are soluble in said compounds.
9. The process according to claim 8, wherein when the fat substance
is solid at room temperature, the fat substance is added to the
pre-emulsion in the molten state or dissolved in a liquid fat
substance.
10. Stable emulsions of a first dispersed phase consisting of a
perfluoropolyether or perfluoropolyethers having perfluoroalkyl end
groups and of a second dispersed phase consisting of one or more
fat substances having a melting temperature not higher than
100.degree. C., said two phases being dispersed in a continuous
phase consisting of one or more polyhydroxylated compounds selected
from glycerol and polyalcohols other than glycerol and saccharides,
containing at least three hydroxyl groups, said emulsions having
the following weight composition:
(a) perfluoropolyether or perfluoropolyethers: 1-50% by weight of
the emulsion, and
(b) polyhydroxylated compound or compounds: 10-95% by weight of the
emulsion, and
(c) fat substance or substances: 10-80% by weight of the emulsion,
and
(d) one or more emulsifiers which are soluble in the
polyhydroxylated compound or compounds: 0.1-10% by weight of the
emulsion,
further comprising up to 20% by weight of the total emulsion of
water or of an alcohol wherein components (a), (b), (c) and (d)
retain their relative proportions.
11. A preparation for cosmetic and dermatological products,
comprising a stable emulsion according to claim 1.
12. The stable emulsions according to claim 1 wherein the
polyhydroxylated compound is glycerol.
13. Stable emulsions of a first dispersed phase consisting of a
perfluoropolyether or perfluoropolyethers having perfluoroalkyl end
groups and of a second dispersed phase consisting of one or more
fat substances having a melting temperature not higher than
100.degree. C., said two phases being dispersed in a continuous
phase consisting of one or more polyhydroxylated compounds selected
from glycerol and polyalcohols other than glycerol and saccharides,
containing at least three hydroxyl groups, said emulsions having
the following weight composition:
(a) perfluoropolyether or perfluoropolyethers: 1-50% by weight of
the emulsion,
(b) polyhydroxylated compound or compounds: 10-95% by weight of the
emulsion,
(C) fat substance or substances: 10-80% by weight of the emulsion,
and
(d) one or more emulsifiers which are soluble in the
polyhydroxylated compound or compounds: 0.1-10% by weight of the
emulsion,
wherein when the polyhydroxylated compounds are solid, the
polyhydroxylated compounds are dissolved in water or in a
hydrophilic solvent so that the concentration of polyhydroxylated
compound is from 50 to 80% by weight of the solution.
Description
The present invention relates to stable emulsions of
perfluoropolyethers having perfluoroalkyl end groups and of fat
substances.
It is known that said perfluoropolyethers exhibit a very high
hydrophobicity and lipophobicity, wherefore it was possible to
prepare stable aqueous emulsions thereof only by by means of
particular combinations of components of the same emulsions.
U.S. Pat. No. 4,803,067 discloses stable emulsions of
perfluoropolyethers having perfluoroalkyl end groups in oil/water
emulsions or water/oil emulsions obtained by using emulsifiers.
These emulsions are utilized, in particular, in lotions and creams
for cosmetology and dermatology, in consideration of the excellent
properties of said perfluoropolyethers in said applications, due to
the particular formation, on the skin, of a water-repellent,
oxygen-permeable and carbon dioxide-permeable protective film,
which permits the normal skin respiration.
European Patent Application No. 390.206 describes stable emulsions
of perfluoropolyethers having perfluoroalkyl end groups in glycerol
or other polyhydroxylated compounds, prepared by using emulsifiers.
In the preparation of cosmetic or dermatological products, the
above said emulsions are added to basic formulations containing the
other components.
So far it was not possible to obtain stable emulsions of
perfluoropolyethers with fat substances, although the need for such
emulsions of anhydrous or substantially anhydrous nature was
strongly felt in the cosmetic and dermatological sectors or in
industrial appliances, wherein said anhydrous or substantially
anhydrous emulsions would have permitted to preserve the
hydrophobic nature of the anhydrous products whereinto they would
have been introduced.
It has now been found that it is possible to obtain stable
emulsions of perfluoropolyethers having perfluoroalkyl end groups
(hereinafter briefly referred to as perfluoropolyethers) and fat
substances if one or more fat substances in the liquid state is or
are added, under stirring, to an emulsion of perfluoropolyether in
glycerol or other polyhydroxylated compounds in the presence of a
surfactant which is soluble in glycerol or in the other
polyhydroxylated compounds.
The existence of said stable emulsions of perfluoropolyethers and
fat substances in glycerol or other polyhydroxylated compounds is
very surprising since it is not possible to emulsify a fat
substance in glycerol or in another polyhydroxylated compound and
it is not possible to emulsify a perfluoropolyether in a fat
substance. It has surprisingly been found that the presence of a
perfluoropolyether in emulsion in glycerol or other
polyhydroxylated compounds makes it possible to emulsify the fat
substance in the perfluoropoly-ether-glycerol system or in the
perfluoropolyether-other polyhydroxylated compounds system.
Thus, it is an object of the present invention to provide stable,
anhydrous or substantially anhydrous emulsions of
perfluoropolyethers and fat substances.
Another object is to provide a process for preparing such
emulsions.
The former object is achieved by the stable emulsions of
perfluoropolyethers having perfluoroalkyl end groups and of fat
substances, conforming to the present invention, which are composed
of:
one or more perfluoropolyethers having perfluoroalkyl end groups:
1-50% by weight,
one or more polyhydroxylated compounds selected from glycerol and
the polyalcohols other than glycerol and the saccharides,
containing at least three hydroxylic groups, said compounds being
dissolved in water or in a hydrophilic solvent when they are solid:
10-95% by weight, including water and hydrophilic solvent, if
any,
one or more fat substances having a melting temperature not higher
than 100.degree. C.: 10-80% by weight,
one or more emulsifiers: 0.1-10% by weight.
By the term fat substance it is meant:
1) a liquid product (oil) insoluble in water and in the
polyhydroxylated compounds as defined hereinabove, and
2) a product which is solid at room temperature (fat), is insoluble
in water and in the polyhydroxylated compounds and has a melting
temperature not exceeding 100.degree. C.
The perfluoropolyethers having perfluoroalkyl end groups, i.e. free
from functional groups, are well-known compounds, which are
described, along with their method of preparation, in several
documents, among which British patent 1,104,482, U.S. Pat. Nos.
3,242,218; 3,665,041; 3,715,378; 4,523,039; European patent
applications 148,482; 151,877 and 191,490 and international patent
applications WO 87/00538 and WO 87/02992. Several
perfluoropolyethers are available on the market under the
trademarks Fomblin.RTM., Galden.RTM., Krytox.RTM. and
Demnum.RTM..
Suitable perfluoropolyethers are the ones characterized by the
presence of one or more repeating perfluorooxyalkylene units:
a) (CF.sub.2 --CF.sub.2 O)
b) (CF.sub.2 O)
c) (C.sub.3 F.sub.6 O), simplified formula for ##STR1## d)
(CF.sub.2 O--CF.sub.2 --CF.sub.2 O) e) (CF.sub.2 --CF.sub.2
--CF.sub.2 O)
f) (CFO)/CF.sub.3 ##STR2## where the R.sub.f "' groups, like or
unlike each other, are a fluorine atom or a perfluoroalkyl group
preferably containing 1 to 3 carbon atoms.
Preferably the perfluoropolyethers suitable for the present
invention exhibit the following individual perfluoro-oxyalkylene
units or the following combinations of perfluoro-oxyalkylene
units:
I) (CF.sub.2 --CF.sub.2 O) and (CF.sub.2 O), these units being
statistically distributed along the perfluoropolyether chain;
or
II) ##STR3## and (CFXO), where X is F or CF.sub.3, said units being
statistically distributed along the chain; or
III) (CF.sub.2 --CF.sub.2 O), ##STR4## and (CFXO), wherein X is F
or CF.sub.3, said units being statistically distributed along the
chain; or
IV) ##STR5## or V) (CF.sub.2 --CF.sub.2 --CF.sub.2 O); or
VI) (CF.sub.2 --CF.sub.2 O); or ##STR6## where the R.sub.f "'
groups, like or unlike each other, are a fluorine atom or a
perfluoroalkyl group preferably containing 1 to 3 carbon atoms;
or
VIII) (CF.sub.2 O--CF.sub.2 --CF.sub.2 O)
Suitable are also the perfluoropolyethers containing
perfluorooxyethane rings ##STR7## wherein T, A, B and R, like or
different from one another, are perfluorooxyalkyl,
perfluoropolyoxyalkyl or perfluoroalkyl radicals preferably
containing 1 to 6 carbon atoms.
Examples of suitable perfluoropolyethers having repeating
perfluorooxyalkylene units are the ones belonging to the following
classes:
A) ##STR8## where: R.sub.f and R'.sub.f, like or unlike each other,
are selected from the group consisting of CF.sub.3, C.sub.2 F.sub.5
and C.sub.3 F.sub.7 ; units C.sub.3 F.sub.6 O
(oxytrifluoromethyltrifluoroethylene), ##STR9## and CF.sub.2 O are
statistically distributed along the chain; a is an integer; b and c
are integers or zero; when the sum (b+c) is other than zero, the
##EQU1## ratio ranges from 5 to 40; B) CF.sub.3 O--(C.sub.2 F.sub.4
O).sub.d (CF.sub.2 O).sub.e --CF.sub.3 where units C.sub.2 F.sub.4
O and CF.sub.2 O are statistically distributed along the chain; d
and e are integers; the d/e ratio varies from 0.3 to 5;
C) CF.sub.3 O--(C.sub.3 F.sub.6 O).sub.f (C.sub.2 F.sub.4 O).sub.g
--(CFXO).sub.h --CF.sub.3 where units C.sub.3 F.sub.6 O, C.sub.2
F.sub.4 O and CFXO are statistically distributed along the chain; X
is F or CF.sub.3 ; f, g and h are integers; the ##EQU2## ratio
ranges from 1 to 50, and the ##EQU3## ratio ranges from 1 to 10; D)
R.sub.8.sup.3 O--(CF.sub.2 CF.sub.2 CF.sub.2 O).sub.j
R.sub..delta..sup.4 g where R.sub..delta..sup.3 and
R.sub..delta..sup.4, like or different from each other, are
--CF.sub.3 or --C.sub.2 F.sub.5 and j is an integer.
The perfluoropolyethers suited to be used in the present invention
have generally a number average molecular weight ranging from 500
to 20,000 and, more commonly, from 1,000 to 10,000.
The polyhydroxylated compounds suited to the present invention are
described more in detail in the cited European patent application
390,206 in the name of the same Applicant, which is incorporated in
the specification of the present invention as a reference.
When the polyhydroxylated compound is solid, it is dissolved in
water or in a hydrophilic solvent. It is advisable to use the
minimum amount of water or of hydrophilic solvent which is
necessary to dissolve the compound.
Suitable hydrophilic solvents are, for example, glycols, glycerol,
lower alcohols, ethereal solvents and diglymes, also admixed with
water.
However, water is usually utilized as a solvent. Suitable are the
concentrated aqueous solutions (syrups) of polyalcohols and
saccharides, which are commercially available.
Usually the concentration of the solutions ranges from 50% to 80%
by weight.
Best preferred polyhydroxylated compounds are glycerine,
diglycerol, triglycerine and tetraglycerine.
The oils and the fats according to the present invention can be of
vegetable, animal, hydrocarbon or synthetic nature. They are in
particular fatty alcohols, acids, esters and amides, silicone oils
and hydrocarbon oils and fats.
The emulsifier shall be soluble in the polyhydroxylated compound.
Among the suitable emulsifiers, the following ones can be cited as
examples:
sodium laurylsulphate,
sulpnosuccinate (sulphosuccinic hemiester),
coco amphocarboxyglycinate,
potassium cetylphosphate,
sodium alkyl-polyoxyethylene-ether carboxylate,
benzalconium chloride,
alkylamidopropylbetaine,
coco amidopropylbetaine.
The emulsions according to the present invention have preferably
the following composition:
perfluoropolyether or perfluoropolyethers: 5-25% by weight;
one or more polyhydroxylated compounds: 10-59% by weight;
fat substance or substances: 35-80% by weight;
emulsifier or emulsifiers: 0.3-3% by weight.
The most preferred emulsions contain from 10 to 40% by weight of
polyhydroxylated compound.
Commonly, the emulsions contain only one perfluoropolyether and
only one polyhydroxylated compound.
Depending on the nature and proportion of the components, the
emulsions of the present invention exhibit a very wide viscosity
range, which makes them suitable for a broad applicative field. The
least viscous emulsions have, for example, a viscosity of 2,000 cps
(centipoises) at 25.degree. C., while the most viscous emulsions
have, for example, a viscosity of 1,000,000 cps or above.
The viscosity increases with the concentration of the fat
substances and of the perfluoropolyethers and when use is made of
more viscous polyhydroxylated compounds.
At equal concentration, also the nature of the fat substances
influences the viscosity.
The viscosity of the emulsions can be lowered, if so desired, by
addition of water or of alcohols. Suitable alcohols are, for
example, alkyl alcohols having 1 to 4 carbon atoms, and ethylene
glycols containing 2 to 4 carbon atoms.
The addition of water or alcohol tends to lower the stability of
the emulsions, wherefore it is not advisable to add more than about
20% thereof, calculated on the total weight of the emulsion.
The minimum added amount of water or alcohol is, for example, equal
to 1%. If water or alcohol is added, the percent amount of the
other components, of course, is reduced, although maintaining
unaltered their reciprocal proportions.
The water- or alcohol-containing emulsions are useful in those
applications in which a low or relatively low viscosity without a
high hydrophobicity is desired.
According to the present invention, stable emulsions are considered
the ones, which do not give rise to phase separation phenomena
after centrifugation at 4,000 rpm for a time of 30 minutes and a
subsequent treatment in oven at 50.degree. C. for a week.
The emulsions according to the present invention can be prepared as
follows: to an emulsion of one or more perfluoropolyethers in one
or more polyhydroxylated compounds containing one or more
emulsifiers which are soluble in said polyhydroxylated compounds
(such emulsion will be briefly referred to as "pre-emulsion") there
are added, under stirring, one or more fat substances in the liquid
state.
The pre-emulsion is at a temperature, which is not critical; in
most cases it is at room temperature.
When the fat substance is solid at room temperature, it is added to
the pre-emulsion in the molten state or dissolved, in particular,
in a liquid fat substance conforming to the present invention,
preferably a hydrocarbon oil, while heating, if necessary, in order
to favour the dissolution.
When the fat substance is added at a temperature above the room
temperature, it is advisable to preheat the pre-emulsion to a
temperature next or equal to the temperature of the fat
substance.
The preparation of the pre-emulsions is described in detail in
European patent application 390,206 already cited herein.
Such emulsions are preparable by adding the perfluoropolyether or
perfluoropolyethers, under stirring, to a solution of one or more
emulsifiers in one or more polyhydroxylated compounds.
At the end of the addition it is advisable to go on stirring at a
lower speed, for example for 30-120 minutes, in order to obtain the
best homogenization.
It is assumed that she outer phase of the emulsions according to
the present invention consists of the polyhydroxylated compound or
compounds, while the perfluoropolyether or perfluoropolyethers and
the fat substance or substances constitute inner dispersed phases.
In fact, these emulsions are dilutable with glycerol and with water
(without having recourse to mechanical stirring), but are not
dilutable with perfluoropolyethers and fat substances (unless
mechanical stirring is utilized). Also the fact that the viscosity
increases as the content of perfluoropolyethers or of fat
substances increases, indicates that these two types of components
form the inner phases.
The emulsions of the present invention have a wide field of uses in
cosmetology and dermatology and in the industrial sector.
The introduction of liposoluble substances into the oily phase
(such as, for example, vitamins or solar filters) or of
glycerol-soluble substances permits to functionalize the cosmetic
and dermatological preparations.
Among the cosmetic applications there are to be cited for example:
barrier creams, sun-preparations, lip-ointments and anhydrous
cosmetics, such as lipsticks and sticks.
Among the dermatological applications there are to be cited, for
example, the skin protective preparations and the
medicament-slow-release preparations.
Among the industrial applications there are to be cited the
lubrication and the water-repellent treatments of textiles and
leather.
The anhydrous nature of the emulsions, or in any case, the presence
therein of little water amounts, makes biologically more stable the
cosmetic and dermatological products prepared with said emulsions.
In fact, said products do not require, usually, the presence of
preservatives. Also the anhydrous nature of the emulsions secures a
higher persistence of said products on the skin. A further
advantage in the same applicative fields consists in the fact that
the emulsions according to the present invention require the
presence of lesser amounts of surfactant than the ones which are
contained in the emulsions of perfluoropolyethers in water/oil or
oil/water emulsions described in the above-cited U.S. Pat. No.
4,803,067.
The following examples are given merely for illustrative purposes
and should not be construed to be a limitation of the scope of the
present invention.
Examples 1 to 33 illustrate various emulsions conforming to the
present invention and the modalities for preparing them. All the
compositions are indicated in % by weight.
The stability test is the one previously described.
The utilized perfluoropolyethers have the structure and the
characteristics indicated hereinbelow:
Fomblin HC/25 ##STR10## n/m=20 to 40 M.W. (number average molecular
weight)=3,200. Galden DO3 the same formula as the preceding product
n/m=20 to 40 M.W.=870
Fomblin HC/R the same formula as the preceding product n/m=20 to 40
M.W.=6,600
Demnum S-65 F(CF.sub.2 --CF.sub.2 --CF.sub.2 O).sub.n CF.sub.2
CF.sub.3 M.W.=4,500
Fomblin Z25 CF.sub.3 --(OCF.sub.2 CF.sub.2).sub.p (OCF.sub.2).sub.q
--OCF.sub.3 p/q=0.6 to 0.7 M.W.=9,400
EXAMPLE 1
______________________________________ Fomblin HC/25 59% Glycerol
29% Texapon N/40* 2% Vaseline oil (density: 0.83) 10%
______________________________________ *sodium lauryl sulphate
(solution at 28%) produced by Henkel.
Into the pre-emulsion of Fomblin HC/25, glycerol and Texapon N/40,
the vaseline oil was added at room temperature, while stirring by
means of a Silverson L/2R turbo-emulsifier at 5,000-6,000 rpm.
Unless otherwise specified, the emulsions illustrated in the
following examples were prepared according to the same
procedure.
The emulsion was stable. Its viscosity, as well as the one of the
emulsions of the subsequent examples, was determined by means of a
Brookfield digital eight-speed viscosimeter, model RTV-II,
following the manufacturer's rules.
Viscosity: 36,600 cps (centipoises) at 25.degree. C. (5 r.p.m.,
impeller 29) .
EXAMPLE 2
______________________________________ Fomblin HC/25 29% Glycerol
59% Texapon N/40 2% Vaseline oil 10%
______________________________________
Viscosity: 2,000 cps (5 rpm, impeller 29) at 25.degree. C. Stable
emulsion.
EXAMPLE 3
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Vaseline oil 39%
______________________________________
Viscosity: 50,000 cps (5 rpm, impeller 29) at 25.degree. C. Stable
emulsion.
EXAMPLE 4
______________________________________ Fomblin HC/25 15% Glycerol
29% Texapon N/40 2% Vaseline oil 54%
______________________________________
Viscosity: 950,000 cps (1 rpm, impeller 29) at 25.degree. C. Stable
emulsion.
EXAMPLE 5
______________________________________ Fomblin HC/25 10% Glycerol
59% Texapon N/40 2% Vaseline oil 29%
______________________________________
Viscosity: 3,100 cps (5 rpm, impeller 29) at 25.degree. C. Stable
emulsion.
EXAMPLE 6
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Silicone oil (350 cps) 39%
______________________________________
Stable emulsion.
EXAMPLE 7
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% ______________________________________
Mixture of 50% of silicone oil and 50% of vaseline oil 39% Stable
emulsion.
EXAMPLE 8
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Abil K4 (volatile silicone) 39%
______________________________________
Stable emulsion.
EXAMPLE 9
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Wheat germ oil 39%
______________________________________
Stable emulsion.
EXAMPLE 10
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Jojoba oil 39%
______________________________________
Stable emulsion.
EXAMPLE 11
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Eutanol G (2-octyl-dodecanol) 39% produced by
Henkel ______________________________________
Stable emulsion.
EXAMPLE 12
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Mirytol (triglyceride of the 39% capric and
caproic acids) produced by Henkel
______________________________________
Stable emulsion.
EXAMPLE 13
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Octyl stearate (Cetiol 868 prod- 39% uced by
Henkel) ______________________________________
Stable emulsion.
EXAMPLE 14
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Olive oil 39%
______________________________________
Stable emulsion.
EXAMPLE 15
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Paraffin C10/C13 39%
______________________________________
Stable emulsion.
EXAMPLE 16
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Ropy vaseline 39%
______________________________________
The ropy vaseline was introduced in the molten state at a
temperature of about 55.degree. C. into the pre-emulsion preheated
to 45.degree. C. Stable emulsion.
EXAMPLE 17
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Ropy vaseline 13% Paraffin C10/C13 26%
______________________________________
The ropy vaseline and the paraffin were premixed before being
introduced into the pre-emulsion. Stable emulsion.
EXAMPLE 18
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Castor-oil 39%
______________________________________
Stable emulsion.
EXAMPLE 19
______________________________________ Fomblin HC/25 20% Glycerol
39% Texapon N/40 2% Linseed-oil 39%
______________________________________
Stable emulsion.
EXAMPLE 20
______________________________________ Fomblin HC/25 14% Glycerol
27% Texapon N/40 2% Vaseline oil 52% Water 5%
______________________________________
Water was added last. Stable emulsion. Viscosity: 37,500 cps at
25.degree. C. (5 rpm, impeller 21).
EXAMPLE 21
______________________________________ Fomblin HC/25 13% Glycerol
27% Texapon N/40 2% Vaseline oil 43% Water 10%
______________________________________
Stable emulsion. Viscosity: 7,000 cps at 25.degree. C. (15 rpm,
impeller 21).
EXAMPLE 22
______________________________________ Fomblin HC/25 12% Glycerol
23% Texapon N/40 2% Vaseline oil 43% Water 20%
______________________________________
Stable emulsion.
EXAMPLE 23
______________________________________ Galden DO3 20% Glycerol 39%
Texapon N/40 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 24
______________________________________ Fomblin HC/R 20% Glycerol
39% Texapon N/40 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 25
______________________________________ Demnum S/65 20% Glycerol 39%
Texapon N/40 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 26
______________________________________ Fomblin Z 25 20% Glycerol
39% Texapon N/40 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 27
______________________________________ Fomblin HC/25 20% Glycerol
39% Coco amidopropylbetaine 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 28
______________________________________ Fomblin HC/25 20% Glycerol
39% Benzalconium 2% chloride (solution at 50% in water) Vaseline
oil 39% ______________________________________
Stable emulsion.
EXAMPLE 29
______________________________________ Fomblin HC/25 20% Diglycerol
39% Texapon N/40 2% Vaseline oil 39%
______________________________________
Highly viscous, stable emulsion. Viscosity: 1,000,000 cps (5 rpm,
impeller 29) at 25.degree. C.
EXAMPLE 30
______________________________________ Fomblin HC/25 20% Sorbitol
(70% in water) 39% Texapon N/40 2% Vaseline oil 39%
______________________________________
Stable emulsion.
EXAMPLE 31
______________________________________ Fomblin HC/25 8% Glycerol
27% Diglycerol 8% Vaselin oil 55% Texapon N/40 2%
______________________________________
Stable emulsion. Viscosity: 180,000 cps (1 rpm, impeller 4) at
20.degree. C.
EXAMPLE 32
______________________________________ Fomblin HC/25 5% Glycerol
30% Amphisol K (*) 2% Cetiol 868 (**) 53% Abil K4 (***) 10%
______________________________________ (*)potassium cetylphosphate
produced by Givaudan (**)octyl stearate produced by Henkel
(***)volatile silicone produced by Tego Cosmetics.
Viscosity: 340,000 cps at 20.degree. C. Stable emulsion.
EXAMPLE 33
______________________________________ Fomblin HC/25 10% Glycerol
20% Amphisol K 3% Cetiol 868 63% Abil K4 4%
______________________________________
This preparation was effected in hot conditions by preheating the
pre-emulsion to about 50.degree. C. since the viscosity increase
which occurs at high oil concentrations makes it difficult to
obtain it in cold conditions.
Viscosity: 500,000 cps at 20.degree. C. Stable emulsion.
EXAMPLE 34
Examples 34 to 37 illustrate, for comparative purposes,
compositions which are not conforming to the present invention.
______________________________________ Glycerol 50% Vaseline oil
49% Texapon N/40 1% ______________________________________
The emulsion was fully unstable, with quick separation when at
rest.
EXAMPLE 35
______________________________________ Fomblin HC/25 20% Vaseline
oil 79% Texapon N/40 1 ______________________________________
The emulsion was fully unstable, with quick separation of Fomblin
HC/25 when at rest.
EXAMPLE 36
______________________________________ Fomblin HC/25 50% Vaseline
oil 49% Texapon N/40 1% ______________________________________
Stability: as in example 35.
EXAMPLE 37
______________________________________ Fomblin HC/25 30% Vaseline
oil 67% Arlacel 989 (*) 3% ______________________________________
(*)ethoxylated fatty acid produced by I.C.I. Stability: as in
example 35.
EXAMPLE 38
This example illustrates a barrier cream and its preparation:
______________________________________ A) glycerine 20% Fomblin
HC/R 10% potassium cetyl phosphate 2% (Amphisol K produced by
Givaudan) B) minerla oil 48% dimethicone 20%
______________________________________
To pre-emulsion A, preheated to about 55.degree. C., phase B was
gradually added under stirring. Stirring was then carried on less
intensely until room temperature was reached.
The cream viscosity was of 290,000 cps (1 rpm, impeller 6) at
20.degree. C.
EXAMPLE 39
This example illustrates a vitaminic hydrating cream, prepared
according to the modalities of example 38:
______________________________________ A) glycerine 30% Fomblin
HC/25 10% potassium cetyl phosphate 2% B) octyl dodcenaol (Eutanol
G produced 50.5% by Henkel) cyclomethicone 5% (Abil K4 produced by
Tego Cosmetics) tocopherol acetate 2% retinyl palmitate 0.5%
______________________________________
The cream viscosity was of 180,000 cps (1 rpm, impeller 6) at
20.degree. C.
EXAMPLE 40
Another vitaminic hydrating cream like the preceding one was
prepared, with the exception that 1% of camomile glycolic extract
was added.
The presence of this little amount of glycol was sufficient to
bring the viscosity from 180,000 cps to 50,000 cps.
EXAMPLE 41
This example relates to a sun-cream prepared as in example 38, with
the only exception that phase B was preheated:
______________________________________ A) glycerine 30% Fomblin
HC/R 10% potassium cetyl phosphate 2% B) octyl stearate 46% ethyl
hexyl p-methoxycinnamate 5% (Parisol MCX produced by Gavaudan)
cyclomethicone 5% "Karite butter" 2%
______________________________________
The cream viscosity was of 480,000 cps (1 rpm, impeller 6) at
20.degree. C.
* * * * *